WO2004018723A1 - Alliage al-cu a haute resistance aux deteriorations - Google Patents
Alliage al-cu a haute resistance aux deteriorations Download PDFInfo
- Publication number
- WO2004018723A1 WO2004018723A1 PCT/EP2003/009539 EP0309539W WO2004018723A1 WO 2004018723 A1 WO2004018723 A1 WO 2004018723A1 EP 0309539 W EP0309539 W EP 0309539W WO 2004018723 A1 WO2004018723 A1 WO 2004018723A1
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- WO
- WIPO (PCT)
- Prior art keywords
- alloy
- product
- rolled
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- product according
- Prior art date
Links
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 78
- 239000000956 alloy Substances 0.000 title claims abstract description 78
- 229910018182 Al—Cu Inorganic materials 0.000 title abstract 2
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 239000004411 aluminium Substances 0.000 claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 229910000881 Cu alloy Inorganic materials 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000005098 hot rolling Methods 0.000 claims description 12
- 229910052726 zirconium Inorganic materials 0.000 claims description 10
- 238000005097 cold rolling Methods 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 230000000171 quenching effect Effects 0.000 claims description 3
- 229910052706 scandium Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910019064 Mg-Si Inorganic materials 0.000 claims 1
- 229910019406 Mg—Si Inorganic materials 0.000 claims 1
- 238000003303 reheating Methods 0.000 claims 1
- 239000011572 manganese Substances 0.000 description 29
- 239000010949 copper Substances 0.000 description 18
- 239000011777 magnesium Substances 0.000 description 16
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 12
- 229910052748 manganese Inorganic materials 0.000 description 12
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 8
- 239000011651 chromium Substances 0.000 description 8
- 229910000838 Al alloy Inorganic materials 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910017818 Cu—Mg Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/12—Alloys based on aluminium with copper as the next major constituent
- C22C21/16—Alloys based on aluminium with copper as the next major constituent with magnesium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/12—Alloys based on aluminium with copper as the next major constituent
- C22C21/18—Alloys based on aluminium with copper as the next major constituent with zinc
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/057—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with copper as the next major constituent
Definitions
- the present invention relates to a high damage tolerant AI-Cu alloy product having a high toughness and an improved fatigue crack growth resistance while maintaining good strength levels, to a method for producing such a rolled high damage tolerant AI-Cu alloy product having a high toughness and an improved fatigue crack growth resistance and further to a rolled alloy sheet product for aeronautical applications. More specifically, the present invention relates to a high damage tolerant Al-Cu-Mg alloy designated by the Aluminium Association ("AA”)2xxx-series for structural aeronautical applications with improved properties such as fatigue crack growth resistance, strength and fracture toughness. The invention also relates to a rolled alloy product which is suitable used as fuselage skin or lower wing skin of an aircraft.
- AA Aluminium Association
- aluminium alloys 2024, 2324 and 2524 are well known heat treatable aluminium alloys which have useful strength and toughness properties in T3, T39 and T351 tempers.
- the design of a commercial aircraft requires various properties for different types of structures on the aircraft. Especially for fuselage skin or lower wing skin it is necessary to have properties such as good resistance to crack propagation either in the form of fracture toughness or fatigue crack growth. At the same time the strength of the alloy should not be reduced. A rolled alloy product either used as a sheet or as a plate with an improved damage tolerance will improve the safety of the passengers, will reduce the weight of the aircraft and thereby improve the fuel economy which translates to a longer flight range, lower costs and less frequent maintenance intervals.
- US-5, 593,516 discloses a high damage tolerant AI-Cu alloy with a balanced chemistry comprising essentially the following composition (in weight %):
- Mn up to 0.8 balance aluminium and unavoidable impurities. It also discloses T6 and T8 tempers of such alloys which gives high strength to a rolled product made of such alloy.
- US-5,897,720 discloses a high damage tolerant AI-Cu alloy with a "2024"- chemistry comprising essentially the following composition (in weight %): Cu 3.8 - 4.9
- the alloy is annealed after hot rolling at a temperature at which the intermetallics do not substantially dissolve.
- the annealing temperature is between 398°C and 455°C.
- US-5,938,867 discloses a high damage tolerant AI-Cu alloy with a "2024"- chemistry comprising essentially the following composition (in weight %):
- EP-0473122 as well as US-5,213,639, disclose an aluminium base alloy comprising essentially the following composition (in weight %): Cu 3.8 - 4.5, preferably 4.0 - 4.5
- Mg 1.2 - 1.8 preferably 1.2 -1.5 Mn 0.3 - 0.9, preferably 0.4 - 0.7
- US-5,213,639 discloses an inter-anneal treatment after hot rolling the cast ingot with a temperature between 479°C and 524°C and again hot rolling the inter-annealed alloy wherein the alloy contains one or more elements from the group consisting of Cr, V, Hf, Cr, Ag and Sc, each within defined ranges.
- Such alloy is reported to have a 5% improvement over the above mentioned conventional 2024-alloy in T-L fracture toughness and an improved fatigue crack growth resistance at certain ⁇ K-levels.
- EP-1170394-A2 discloses an aluminium sheet product with improved fatigue crack growth resistance having an anisotropic microstructure defined by grains having an average length to width aspect ratio of greater than about 4 to 1 and comprising essentially the following composition, (in weight %):
- Yet a further object of the present invention is to provide rolled aluminium alloy sheet products and a method for producing those products so as to provide structural members for aircrafts which have an increased resistance to fatigue crack growth and to provide an improved fracture toughness while still maintaining high levels of strength.
- FCGR fatigue crack growth rate
- Fig. 1 shows the fatigue crack growth properties versus a 2524 reference alloy
- Fig. 2 shows the Kahn-tear versus yield strength properties compared to 2024-
- Fig. 3 shows the Kahn-tear versus yield strength properties as shown in Fig. 2 but in average L-T and T-L direction.
- a high damage tolerant AI-Cu alloy having a high toughness and an improved fatigue crack growth resistance by maintaining high levels of strength which comprises essentially the following composition (in weight %):
- Mn >0 - 0.50, and preferably > 0.15 - 0.50 Cr ⁇ 0.15
- Si ⁇ 0.15, preferably ⁇ 0.10, and Mn-containing dispersoids and Zr-containing dispersoids, the balance essentially aluminium and incidental elements and impurities, wherein the Mn- containing dispersoids are at least partially replaced by Zr-containing dispersoids.
- the alloy contains Mn-containing dispersoids and Zr-containing dispersoids.
- the alloy of the instant invention in a T3 temper has significant improved high damage tolerance properties by lowering the amount of manganese and by partially replacing manganese-containing dispersoids by zirconium containing dispersoids. At the same time it is important to carefully control the chemistry of the alloy.
- the main improvement of the alloy according to the present invention is an improved fatigue crack growth resistance at the lower ⁇ K-values which leads to significant longer lifetimes.
- the balance of high damage tolerance properties and mechanical properties of the alloy of the present invention is better than the balance of conventional 2024 or 2524-T3 alloys.
- the toughness levels are equal or better to 2524 alloy levels. It has been found that the high damage tolerance properties such as fracture toughness or strength may be further improved by adding zirconium.
- the amount (in weight %) of manganese is preferably in a range of 0.20 to
- Mn contributes to or aids in grain size control during operations.
- the preferred levels of manganese are lower than those conventionally used in conventional AA2x24 alloys while still resulting in sufficient strength and improved damage tolerance properties.
- the chemical composition of the alloy of the present invention preferably meets the proviso that Zr > 0.09 when Mn ⁇ 0.45 and Cu > 4.0.
- the amount (in weight %) of copper is in a range of 4.0 to 4.4, preferably in a range of 4.1 to 4.3. Copper is an important element for adding strength to the alloy rolled product. It has been found that a copper content of 4.1 or 4.2 results in a good compromise in strength, toughness, formability and corrosion performance while still resulting in sufficient damage tolerance properties.
- the preferred amount (in weight %) of magnesium is in a range of 1.0 to 1.4, most preferably in a range of 1.1 to 1.3. Magnesium provides also strength to the alloy rolled product.
- the preferred amount (in weight %) of zirconium is in a range of 0.09 to 0.15 thereby partially replacing Mn-containing dispersoids.
- the balance of manganese and zirconium influences the recrystallisation behaviour. Throughout the addition of zirconium more elongated grains may be obtained which also results in an improved fatigue crack growth resistance.
- Zirconium may also be at least partially replaced by chromium wherein [Zr] + [Cr] ⁇ 0.20.
- Preferred amounts (in weight %) of chromium and zirconium are in a range of 0.05 to 0.15, preferably in a range of 0.10 to 0.13.
- the balance of zirconium and chromium as well as the partial replacement of Mn- containing dispersoids and Zr-containing dispersoids result in an improved recrystallisation behaviour and more elongated grains.
- a preferred alloy composition of the present invention comprises the following composition (in weight %):
- Another preferred alloy according to the present invention consists of the following composition (in weight %):
- an alloy according to the present invention consists of the following composition (in weight %):
- the balance in the rolled alloy product according to the invention is aluminium and inevitable impurities and incidental elements. Typically, each impurity element is present at 0.05% maximum and the total of impurities is 0.20% maximum. Preferably the alloy product is substantially Ag-free.
- the alloy rolled products have a recrystallised microstructure meaning that 75% or more, and preferably more than 80% of the grains in a T3 temper, e.g. T39 or T351 , are recrystallised.
- the grains have an average length to width aspect ratio of smaller than about 4 to 1 , and typically smaller than about 3 to 1 , and more preferably smaller than about 2 to 1.
- the alloy according to the present invention may further comprise one or more of the elements Zn, Hf, V, Sc, Ti or Li, the total amount less than 1.00 (in weight %). These additional elements may be added to further improve the balance of the chemistry and enhance the forming of dispersoids.
- the invention provides a method for producing a rolled high damage tolerant AI-Cu alloy product having a composition as set out above and having a high toughness and an improved fatigue crack growth resistance according to the invention comprises the steps of: a) casting an ingot having a composition as set out above and set forth in the claims, b) homogenizing and/or pre-heating the ingot after casting, c) hot rolling the ingot and optionally cold rolling into a rolled product, d) solution heat treating, e) quenching the heat treated product, f) stretching the quenched product, and g) naturally ageing the rolled and heat-treated product.
- the ingot After hot rolling the ingot it is possible to anneal and/or re-heat the hot rolled ingot and again hot rolling the rolled ingot. It is believed that such re-heating or annealing enhances the fatigue crack growth resistance by producing elongated grains which - when recrystallized - maintain a high level of toughness and good strength. It is furthermore possible to conduct a surface heat treatment between hot rolling and cold rolling at the same temperatures and times as during homogenisation, e.g. 1 to 5 hours at 460°C and about 24 hours at 490°C.
- the hot rolled ingot is preferably inter-annealed before and/or during cold rolling to further enhance the ordering of the grains.
- Such inter-annealing is preferably done at a gauge of about 4.0 mm for one hour at 350°C. Furthermore, it is advisable to stretch the rolled and heat- treated product in a range of 1 to 5%, preferably in a range of 1 to 3%, and then naturally aging the stretched product for more than 5 days, preferably about 10 to 20 days, and more preferably for 10 to 15 days, to provide a T3 temper condition, in particular a T351 temper condition.
- the present invention provides a high damage tolerant rolled AI-Cu alloy sheet product which has high toughness and an improved fatigue crack growth resistance with the above described alloy composition which is preferably produced in accordance with the above described method.
- Such rolled alloy sheet product has preferably a gauge of around 2.0 mm to 12 mm for applications such as fuselage skin and about 25 mm to 50 mm for applications such as lower-wing skin.
- the present invention thereby provides an aircraft fuselage sheet or an aircraft lower-wing member sheet with improved high damage tolerance properties.
- the sheet may be unclad or clad, with preferred cladding layer thickness of from about 1 to about 5 percent of the thickness of the sheet.
- Fig. 1 shows the fatigue crack growth properties versus a 2524 reference alloy
- Fig. 2 shows the Kahn-tear versus yield strength properties compared to 2024-
- Fig. 3 shows the Kahn-tear versus yield strength properties as shown in Fig. 2 but in average L-T and T-L direction.
- the alloys have been processed to a 2.0 mm sheet in the T351 temper.
- the cast ingots were homogenized at about 490°C, and subsequently hot rolled at about 410°C.
- the plates were further cold rolled, surface heat treated and stretched by about 1%. All alloys have been tested after at least 10 days of natural aging.
- the Kahn-tear versus yield strength properties of the alloys according to the present invention are better than those of conventional 2024-T351 in commercially available form or pure form. Furthermore, the preferred minimum level of manganese is in between 0.21 and 0.31 while at a level of 0.21 the strength level is still good.
- FCGR fatigue crack growth rate
- the preferred amount of Mn is in a range of 0.25 to 0.45 (in weight %) and the preferred range of Zr is in between 0.09 and 0.15 (in weight %).
- Copper is most preferably present in an amount below 4.3 and magnesium is preferably present in an amount below 1.3 (in weight %).
- alloys 3 and 5 have a significantly improved lifetime over conventional AA2024 alloys preferably at ⁇ K-levels in a range of 5 to 15 MPa m. Hence, the fatigue crack growth resistance at those lower ⁇ K-values results in significant longer lifetimes of the alloy and enhances its usefulness for aeronautical applications.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metal Rolling (AREA)
- Laminated Bodies (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA2493403A CA2493403C (fr) | 2002-08-20 | 2003-08-19 | Alliage al-cu a haute resistance aux deteriorations |
GB0502069A GB2406576B (en) | 2002-08-20 | 2003-08-19 | High damage tolerant Al-Cu alloy |
BRPI0313640-0A BR0313640B1 (pt) | 2002-08-20 | 2003-08-19 | Processo para a produção de liga de Al-Cu de alta tolerância a dano |
AU2003264120A AU2003264120A1 (en) | 2002-08-20 | 2003-08-19 | HIGH DAMAGE TOLERANT Al-Cu ALLOY |
DE10393144T DE10393144T5 (de) | 2002-08-20 | 2003-08-19 | Al-Cu Legierung mit hoher Toleranz gegenüber Beschädigungen |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP02078443 | 2002-08-20 | ||
EP02078443.5 | 2002-08-20 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2004018723A1 true WO2004018723A1 (fr) | 2004-03-04 |
Family
ID=31197925
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2003/009539 WO2004018723A1 (fr) | 2002-08-20 | 2003-08-19 | Alliage al-cu a haute resistance aux deteriorations |
Country Status (9)
Country | Link |
---|---|
US (2) | US7323068B2 (fr) |
CN (1) | CN100340687C (fr) |
AU (1) | AU2003264120A1 (fr) |
BR (1) | BR0313640B1 (fr) |
CA (1) | CA2493403C (fr) |
DE (1) | DE10393144T5 (fr) |
FR (1) | FR2843755B1 (fr) |
GB (1) | GB2406576B (fr) |
WO (1) | WO2004018723A1 (fr) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2007048565A1 (fr) * | 2005-10-25 | 2007-05-03 | Aleris Aluminum Koblenz Gmbh | Alliage al-cu-mg adapte a une application aerospatiale |
US7323068B2 (en) | 2002-08-20 | 2008-01-29 | Aleris Aluminum Koblenz Gmbh | High damage tolerant Al-Cu alloy |
US7604704B2 (en) | 2002-08-20 | 2009-10-20 | Aleris Aluminum Koblenz Gmbh | Balanced Al-Cu-Mg-Si alloy product |
EP2458026A1 (fr) * | 2004-07-15 | 2012-05-30 | Alcoa Inc. | Alliages de la série 2000 présentant une tolérance aux dommages accrus d'efficacité pour des applications aérospatiales |
CN105239029A (zh) * | 2015-10-23 | 2016-01-13 | 苏州有色金属研究院有限公司 | 控制Al-Cu-Mg-Mn合金中含Mn相均匀弥散析出的热处理方法 |
CN105463349A (zh) * | 2015-11-24 | 2016-04-06 | 苏州有色金属研究院有限公司 | 改善2×××-t3板疲劳裂纹扩展速率的热处理方法 |
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WO2004005562A2 (fr) * | 2002-07-09 | 2004-01-15 | Pechiney Rhenalu | Alliages a base d'aluminium, de cuivre et de magnesium (alcumg), hautement insensibles aux defaillances et utilisables comme elements de structure d'un aeronef |
US7494552B2 (en) * | 2002-08-20 | 2009-02-24 | Aleris Aluminum Koblenz Gmbh | Al-Cu alloy with high toughness |
US20070151637A1 (en) * | 2005-10-28 | 2007-07-05 | Aleris Aluminum Koblenz Gmbh | Al-Cu-Mg ALLOY SUITABLE FOR AEROSPACE APPLICATION |
US20110176957A1 (en) * | 2008-07-09 | 2011-07-21 | Yun Che | High strength casting aluminum alloy material |
CA2750394C (fr) * | 2009-01-22 | 2015-12-08 | Alcoa Inc. | Alliages ameliores d'aluminium-cuivre contenant du vanadium |
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CN105441839B (zh) * | 2016-01-12 | 2017-08-08 | 苏州有色金属研究院有限公司 | 提高2×××系铝合金板材抗疲劳损伤性能的加工工艺 |
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CN117551950B (zh) * | 2024-01-11 | 2024-04-09 | 中北大学 | 一种具有优异长期热稳定性的Al-Cu-Mg-Ag合金及其热处理工艺 |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7323068B2 (en) | 2002-08-20 | 2008-01-29 | Aleris Aluminum Koblenz Gmbh | High damage tolerant Al-Cu alloy |
US7604704B2 (en) | 2002-08-20 | 2009-10-20 | Aleris Aluminum Koblenz Gmbh | Balanced Al-Cu-Mg-Si alloy product |
US7815758B2 (en) | 2002-08-20 | 2010-10-19 | Aleris Aluminum Koblenz Gmbh | High damage tolerant Al-Cu alloy |
EP2458026A1 (fr) * | 2004-07-15 | 2012-05-30 | Alcoa Inc. | Alliages de la série 2000 présentant une tolérance aux dommages accrus d'efficacité pour des applications aérospatiales |
WO2007048565A1 (fr) * | 2005-10-25 | 2007-05-03 | Aleris Aluminum Koblenz Gmbh | Alliage al-cu-mg adapte a une application aerospatiale |
CN105239029A (zh) * | 2015-10-23 | 2016-01-13 | 苏州有色金属研究院有限公司 | 控制Al-Cu-Mg-Mn合金中含Mn相均匀弥散析出的热处理方法 |
CN105463349A (zh) * | 2015-11-24 | 2016-04-06 | 苏州有色金属研究院有限公司 | 改善2×××-t3板疲劳裂纹扩展速率的热处理方法 |
Also Published As
Publication number | Publication date |
---|---|
FR2843755B1 (fr) | 2007-01-19 |
GB2406576B (en) | 2006-03-22 |
DE10393144T5 (de) | 2005-08-18 |
CA2493403A1 (fr) | 2004-03-04 |
US20040099353A1 (en) | 2004-05-27 |
CN100340687C (zh) | 2007-10-03 |
US20080121317A1 (en) | 2008-05-29 |
AU2003264120A1 (en) | 2004-03-11 |
GB0502069D0 (en) | 2005-03-09 |
CN1675390A (zh) | 2005-09-28 |
FR2843755A1 (fr) | 2004-02-27 |
BR0313640A (pt) | 2005-06-21 |
US7323068B2 (en) | 2008-01-29 |
US7815758B2 (en) | 2010-10-19 |
BR0313640B1 (pt) | 2014-06-10 |
CA2493403C (fr) | 2012-11-27 |
GB2406576A (en) | 2005-04-06 |
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